Extraction of sugar from cane molasses and the like



cose reaction pro ucts until after the Patented 0a. 2a 1932 UNIT DSTATES PATENT OFFICE enonenr. mums, or currency. Louisiana, in am: it.manna, or unwax,

NEW JERSEY, ASSIGII'OIBB 1'0 mar-Amman SUGAR N. Y, A CORPORATION 0! NEWmun comm, 0] m YORK.

nx'rnaorron or soon m! can lromssxs m m m Illa Drawing.

This invention relates to the extraction of sugar from cane molasses andthe like.

The recovery of sugar from beet molasses by preci itation with bariumalkaline compounds as been practiced successfully but difiiculties havebeen experienced in applying a similar method to cane molasse owin tothe resence of glucose therein. A thou it has on recognized that bariumalkaline compounds will react with and destroy glucose, it has beenthought necessa in order to avoid the diiliculties caused by t epresence of the glucose, to apply a preliminary step in the treatment ofcane molasses before precipitating sugar therefrom. Thus, it has beensuggested to regulate and reduce the propor tion of glucosepresent as apreliminary step, or to precipitate the glucose by means of beriumsilicate and to remove it as a preliminary ste a e have invented amethod b which sugar may be successfully extracted in cane molasses bybarium precipitation without any preliminary step. Our method eliminatesthe ifliculties previously encountered by pre venting the preci itationof the bariumlureci' itated su ar has been removed from the so ution byltration. We have discovered that the glucose decom osition productsformed by the reaction of arium with glucose may be held 1n solution, sothat they do not contammate the precipitated sugar or interfere with thefiltration, by keeping the solution from barium silicate and maintaininin it an alkaline concenration in excess of ve per r excess of five percent of the total water ent in the mixed sugar and barium h droxide centand etion of the filtration.

Our process may be carried out by adding to acane molasses, or any sugarsolution con. taming glucose, a barium hydroxide solution free frombarium silicate and containing sailicient barium to react with anddestro all the glucose present, and to unite with all e su r present asbarium saccharate and, in addition, an excess of barium hydroxide which,when figured in non-hydrollzed. form BaO, is in ressolutions. Forgreatest efliciency, afoxcess preferably at least six per cent until thecomp Application ma Inventor a. me. lerlal 10,409,.

barium h droxide, figured in non-hydrolized form, Bag, should be notless than six per cent of the total water present and the tem rature ofthe mixed solution should be maintained from at to C. v

The sugar is precipitated as barium saccha rate, and the variouscompounds formed by reaction of the barium with the glucose aremaintained in solution. The barium saccharate precipitate is thenseparated by filtration, from the mother liquor which contains theglucose decom ition roducts and the excess of dissolved arium a kali.The filtration may easily be accomplished owing to the absence ofprecipitated g ucose decomposition roducts which, because of theircolloidal orm, have heretofore rendered such filtration of cane molassesdiflicult. In order to secure a complete separation of the barium sacchal he d in solution in the alkaline mother liquor.

The saccharate filter cake may be treated in any usual manner to releaseand recover the an r contained therein.

e mother liquor is treated with sulphurous acid, or other mineral acidto recover the barium which is contained therein both in the form ofdissolved alkaliand in the form of salts of organic acids produced bythe decomposition of t e glucose. The latter part of the barium cannotbe released by weak acids, such as carbonic acid. The barium isrecovered in the form of an insoluble salt of the rfiineral acid used,for example, as barium sul ite,

ur method may be successfully applied to any cane molasses, or any othersugar solution containing glucose, regardless of theratio which thesucrose and glucose are present 1n the molasses or solution. In order toapply our method to any speciflecane moi, or

other solution, the sugar, glucose-and water contents of the molasses,or solution, must first be determined. When these are known, thequantity of barium necessa may be determined approximatclyb the ollowlngempirical rule: Six atoms 0 barium for each five molecules of sucrose,plus two atoms of barium for each one molecule of glucose.

The necessary concentration of the barium hydroxide solution dependsupon the water content of the molasses, that is to say, the greateramount of water in the molasses, the greater must be the concentrationof the barium solution in order that the excess barium hydroxide maymaintain the required percentage of alkalinity in the mixed solutionsafter the reactions of the barium with the lucose and sucrose. Incommercial practice, the desired alkaline concentration in the mixedsolutions may most easily be obtained by using a heavy molasses (57 B.or allow) and a strong barium hydroxide solution, preferably abouttwenty per cent.

The barium hydroxide solution should consist entirely, or in large part,of barium oxide dissolved in water. We have discovered, however, thatequally good results may be obtained by dissolving in water a mixture ofbarium oxidc'and barium sulphide, provided that the barium sulphide doesnot amount to over twenty per cent of the mixed compounds.

A specific example of our method is as follows:

A typical cane molasses is found by analysis to have the followingcomposition Per cent Sucrose content 4---..-

Glucose content Water content 25 Impurities (solid non-sugars) 20 By theempirical rule above given, the

Percent Barium oxide, BaO

Barium sulphide, BaS 3 Water Each pound of this solution contains 0.1774pound of barium.

To comply with the empirical rule given above, this barium solution ismixed with a the cane molasses in the proportion of 2.42

pounds to 1 pound, both the molasses and the solution being maintainedat a temperature of from to C. Barium saccharate 'phide,

precipitates at once in an easily filterable orm. The mother liquor isfound to have an alkaline concentration (determined as the ratio ofbarium oxide, 3110, plus barium sulper cent, which is sufficient tomaintain the gluzose decomposition products in solution since no bariumsilicate is present in the solution.

The barium saccharate precipitate is .filtered out and washed with aseven er cent barium alkaline solution until free rom all traces of themother liquor. It is then subjected to further washings and isdecomposed for a recovery of the sugar b known methods. The mgtherliquor an the first wash water are treated with sulphurous acid, orother mineral acid, to recover the barium contained in them.

What is claimed is:

1. A method for extracting sugar from a sugar solution containingglucose which comprises mixing with said solution a barium hydroxidesolution free from barium silicate quantitatively with the glucose andwith the sugar and, in addition, an excess of barium hydroxide equal,when figured in non-hydrolized form, BaO, to not less than five per centof the water in the mixed solutions, so as to destroy the glucose, toprecipitate the sugar as barium 'saccharate and to maintain the glucosedecomposition products in solution, and separating the sugar-containingrecipitate from the mother liquor containmg the glucose decompositionproducts by filtration.

2. A method for extracting sugar from a sugar solution containingglucose, which comprises mixing with said solution a barium hydroxidesolution free from barium silicate and containing sufiicient barium tocombine quantitatively with the glucose and with theQsugar and, inaddition, an excess of barium hydroxide equal, when figured innon-hydrolized form', BaO, to at leastsix per cent of the water in themixed solutions, so as to destroy the glucose, to precipitate the sugaras barium saccharate and to maintain the glucose decom osition productsin solution, and separating the sugar-containing precipitate from themother liquid containmg the glucose decomposition products byfiltration.

3. A method for extracting sugar from a sugar solution containingglucose, which comprises mixing with said solution a'solution of bariumalkaline compounds free from barium silicate and containing sufficientbarium to combine quantitatively with the glucose and with the sugarand, in addition, an excess of dissolved barium alkaline compoundsequal, when figured in non-hydrolized form, to not less than five percent of B118, to the water present) of 6.67-

90 and containing suflicient barium to combine the water in the mixedsolutions at least eight per cent of the barium alkaline, comconsistingof dissolved barium oxide, so as to destroy t e glucose, to precipitatethe sugar as barium saccharate and to maintain the glucose decom itionproducts in solution, and separating the sugar-containing precipitatefrom the mother liquor containmg t e glucose decomposition products byfiltration.

4. A method for extracting sugar from a sugar solution containingglucose, which cpmprises mixin with said solution a solution of barium aslim com unds free from barium silicate and contaimng suflicient bariumto combine quantitatively with the glucose and with the sugar and,in'addition, an excess of dissolved barium alkaline compounds equal,when figuredin non-hydrolized o glucose decomposition products insolution,

sugar solution containin comprises mixin with said solution a solu-"destroy the glucose, to precipitate and separating the sugar-containingpreci itate from the mother liquor containing t e glucose decom ositionproducts by filtration.

5. A meth for extracting sugar from a sugar solution containing glucose,which comprises mixi with said solution a solution of barium a alinecompounds freefrom barium silicate and containin 'suflicient barium tocombine quantitative y withthe glucose and with the sugar and, inaddition, an excess of dissolved barium alkaline com unds equal, whenfigured in non-hydrozed form, to at least six per centv of the water inthe'mixed solutions approximately eight -five per cent of the bariumalkaline COII'liPOIIIIdS consisting of dissolved barium oxi e andapproximately fifteen r cent consisting of dissolved barium sulp do soas to the sugar as barium saccharate and to maintain the glucosedecomposition products in solution, and separating the sugar-containingpreci itate from the mother liquor containing t e glucose decom itionproducts by filtration. 6. "A metho for extracting sugar from a glucose,which tion of alkaline arium compounds consistin principally of bariumhydroxide and in s cient quantity and suflicient concentration toprovide barium to react quantitativel with the glucose and the sugarand,in addition, to maintain an alkalinity of not less than five. per centin the mixed solution after the barium has reacted gwith. the glucoseand the sugar, so as to destroy the glucose, to precipitate the sugar asbarium sacchiarate containin and to'maintainthe glucose decompositionproducts in solution, separating the'su r-: precipitate from 'themo erliquorb tration, and washing the precipitate wit a solution containingnot less than live per cent of dissolvedbarium alkaline compounds tofree the precipitatesfrom all traces of the inotherliquor and theglucose decomposition products containedtherein.

, 7. A method for extracting sugar from a sugar solution containingglucose, which com 1 prises mixin with said solution a solution ofalkaline barium comgounds consisting principally of barium hy roxide andin suflic'ient quantity and suflicient concentration to provide bariumto react quantitatively with the glucose and the su er and, in a dition,to

maintain an alkalinity of six and one-half per cent in the mixed soution after the barium has reacted with the glucose and the sugar, so asto destroy the glucose, to precipitate the sugar as bariumsaccharate'and to maintainthe glucose decomposition products insolution, 'se arating the sugar-containing precipitate m the motherliqudr by filtration,

and washing the precipitatte with a solution containing six and one-ha fper cent of dissolved barium alkaline compounds to free the precipitatesfrom all traces of the mother liquor and the glucose decompositionproducts contained therein.

8. A method for extracting sugar from a concentrated sugar solutioncontaining known quantities 0 sucrose and glucose which comprises mi ingwith said solution,

a concentrated solution of bariumflalkaline compounds consisting princially of barium hydroxide and free from barium silicate and containingsix atoms of barium'for each five molecules of sucrwe in the su garsolution and, in addition, two atoms of barium for each molecule ofglucose in the sugar solution, so

as to destroy the glucose, to precipitate the sugar as barium saccharateand to maintain the glucose decomposition products in solution, andseparating the sugar-containing precipitate from the mother liquorcontaining the glucose decomposition products, by filtration.

9. A method for extracting sugar from a cane molasses of a concentrationabove 35 B., which comprises mixing with said molasses a solutioncontaining over fifteen per cent of dissolved barium alkaline compoundsconsisting principally of barium hydroxide and in a quantity sufiicientto provide six atoms of barium for each five molecules of sucrose in themolasses and, in addition, two atoms of barium for each molecule ofglucose in the molasses, so as to destroy the glucose, to precipitatethe sugar as barium'aacchtr ate and to maintain the glucose decom itionproducts in solution, and separating the sugar-containing precipitatefrom the mother 4 assume liquor containing the glucose decompositionproducts, by filtration.

10. A method for extracting sugar from a cane molasses of aconcentration of 37 B., which comprises mixing with said molasses asolution containing twenty per cent of dissolved barium alkaline comounds consisting principally of barium hy roxide and in a quantitysufiicient to provide six atoms of barium for each five molecules ofsucrose in the molasses and, in addition, two atoms of barium for eachmolecule of glucose i in the molasses, so as to destroy the glucose, toprecipitate the sugar as barium saccharate and to maintain the glucosedecom osition products in solution, and separating the sugar-containingprecipitate from the mother i liquor containing the glucosedecomposition products, by filtration.

11. A method for extractin sugar from a sugar solution containing gucose, which comprises mixing with said solution a barium hydroxidesolution free from barium silicate and containing suilicient barium toreact with the glucose to form barium salts of organic acids, to reactwith the sucrose to form insoluble barium saccharate, and, in addition,an excess of barium hydroxide equal, when figured in non-hydrolizedform, 13:10, to not less than five per cent of the water of the mixedsolutions, so as to maintain the bariumglucose reaction products insolution, filtering the barium saccharate from the solution, and thentreating the solution with a mineral acid to decompose thebarium-glucose reaction products and recover the barium containedtherein as the barium salt of said mineral acid.

In testimony whereof we have hereunto set our hands.

GEORGE P. MEADE. RALPH N. TRAXLER.

CERTIFICATE OF CORRECTION.

PatentNo. 1,884,798. October 25, 1932.

GEORGE P. MEADE ET AL.

it is hereby certified that error appears in the printed specificationof the above numbered patent requiring correction as follows: Page 2.line 12, liter "bariun1 insert the word "hydroxide"; and line 19, for"57" read "37"; and that the said Letters Patent should be read withthese corrections therein that the same may conform to the record of thecase in the Patent Office.

Signed and sealed this 20th day of December, A. D. 1932.

M. J. Moore.

(Seal) Acting Commissioner of Patents.

4 assume liquor containing the glucose decomposition products, byfiltration.

10. A method for extracting sugar from a cane molasses of aconcentration of 37 B., which comprises mixing with said molasses asolution containing twenty per cent of dissolved barium alkaline comounds consisting principally of barium hy roxide and in a quantitysufiicient to provide six atoms of barium for each five molecules ofsucrose in the molasses and, in addition, two atoms of barium for eachmolecule of glucose i in the molasses, so as to destroy the glucose, toprecipitate the sugar as barium saccharate and to maintain the glucosedecom osition products in solution, and separating the sugar-containingprecipitate from the mother i liquor containing the glucosedecomposition products, by filtration.

11. A method for extractin sugar from a sugar solution containing gucose, which comprises mixing with said solution a barium hydroxidesolution free from barium silicate and containing suilicient barium toreact with the glucose to form barium salts of organic acids, to reactwith the sucrose to form insoluble barium saccharate, and, in addition,an excess of barium hydroxide equal, when figured in non-hydrolizedform, 13:10, to not less than five per cent of the water of the mixedsolutions, so as to maintain the bariumglucose reaction products insolution, filtering the barium saccharate from the solution, and thentreating the solution with a mineral acid to decompose thebarium-glucose reaction products and recover the barium containedtherein as the barium salt of said mineral acid.

In testimony whereof we have hereunto set our hands.

GEORGE P. MEADE. RALPH N. TRAXLER.

CERTIFICATE OF CORRECTION.

PatentNo. 1,884,798. October 25, 1932.

GEORGE P. MEADE ET AL.

it is hereby certified that error appears in the printed specificationof the above numbered patent requiring correction as follows: Page 2.line 12, liter "bariun1 insert the word "hydroxide"; and line 19, for"57" read "37"; and that the said Letters Patent should be read withthese corrections therein that the same may conform to the record of thecase in the Patent Office.

Signed and sealed this 20th day of December, A. D. 1932.

M. J. Moore.

(Seal) Acting Commissioner of Patents.

